Ethanol → HCID 136638011, compound

HRID 2414441Notes

Reaction equation

HRID 2414441 reaction equation
[OH:1][C:2]1[C:7]2[CH:8]=[CH:9][C:10]([O:13][CH:14]3[CH2:19][CH2:18][CH2:17][CH2:16][O:15]3)=[C:11]([CH3:12])[C:6]=2[O:5][C:4](=[O:20])[C:3]=1[CH:21]=O.Cl.[CH3:24][O:25][NH2:26].C([O-])(=O)C.[K+].C(O)C>ClCCl.O>[OH:1][C:2]1[C:7]2[CH:8]=[CH:9][C:10]([O:13][CH:14]3[CH2:19][CH2:18][CH2:17][CH2:16][O:15]3)=[C:11]([CH3:12])[C:6]=2[O:5][C:4](=[O:20])[C:3]=1[CH:21]=[N:26][O:25][CH3:24]

Participants

7

Reactant 4

HCID 702EthanolHCID 517044Potassium AcetateHCID 521874O-Methylhydroxylamine hydrochlorideHCID 135673954HCID 135673954, compound

Product 1

HCID 136638011HCID 136638011, compoundYield 86.7%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6344DichloromethaneSolvent

Procedure

A mixture containing 2.0 g of the product prepared in Stage A, 1.08 g of methoxyamine hydrochloride, 1.93 g of potassium acetate and 20 ml of ethanol is heated under reflux for 1 hour. After evaporating to dryness, the product obtained is dissolved in a mixture of dichloromethane and water (100 ml-100 ml), washed with a dilute solution of sodium acid phosphate and dried. After evaporation, the residue is triturated under ultrasound in the presence of ethyl ether, separated and dried. 1.90 g of product is obtained.

Workup

  1. temperatureis heated
  2. temperatureunder reflux for 1 hour
  3. customAfter evaporating to dryness
  4. customthe product obtained
  5. washwashed with a dilute solution of sodium acid phosphate
  6. customdried
  7. customAfter evaporation
  8. customthe residue is triturated under ultrasound in the presence of ethyl ether
  9. customseparated
  10. customdried

Sources & evidence

ORD record
ord-1e905f8564da46b5aa3c9a130e24d907
Source dataset
uspto-grants-2004_11
Patent number
US06812331B2

Reaction notes

Loading…